Cano J P, Baille A M, Viala A
Arzneimittelforschung. 1975 Jul;25(7):1012-6.
A gaschromatographic assay method is described for the determination of Ro 5-3350 (bromazepam) using Ro 5-4547 (methylbromazepam) as internal standard. After alkaline ether extraction the bromazepam and methylbromazepam obtained from sulfuric acid reextraction are hydrolyzed to ABBP and to MABBP, respectively. After neutralization, the bromo-pyridine-benzophenones are extracted with ether and dissolved in hexane after evaporation of the ether. Under the described gaschromatographic conditions it was found that MABBP and ABBP have retention times of 10.5 and 12.5 min, respectively. The limit of sensitivity is situated at 5 ng/ml of plasma. The specificity is satisfactory since the metabolite which might have interfered (hydroxy-3-bromazepam) appears only at very low concentrations in the blood. The linearity of the calibration curve was confirmed for plasma concentrations up to 100 ng/ml.
描述了一种气相色谱测定方法，以Ro 5-4547（甲基溴西泮）作为内标物来测定Ro 5-3350（溴西泮）。经碱性乙醚萃取后，从硫酸再萃取中获得的溴西泮和甲基溴西泮分别水解为ABBP和MABBP。中和后，用乙醚萃取溴吡啶二苯甲酮，乙醚蒸发后将其溶于己烷。在所描述的气相色谱条件下，发现MABBP和ABBP的保留时间分别为10.5分钟和12.5分钟。灵敏度极限为血浆5 ng/ml。特异性令人满意，因为可能产生干扰的代谢物（羟基-3-溴西泮）在血液中的浓度非常低。校准曲线在血浆浓度高达100 ng/ml时的线性得到了证实。
